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Rare-earth complex coated nanometer hollow SiO2, coated -earth complex and preparation method of coated -earth complex

A complex and rare earth technology, applied in chemical instruments and methods, nanotechnology, nanotechnology, etc., can solve problems such as unreported, and achieve the effect of saving rare earth resources, saving rare earth consumption, and high fluorescence intensity

Inactive Publication Date: 2019-03-22
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] However, although the technology of this kind of silica-coated rare earth complex has been reported, the search found that the rare earth complex coated nano-hollow SiO 2 And the patent of coated rare earth complex and its preparation method has not been reported yet

Method used

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  • Rare-earth complex coated nanometer hollow SiO2, coated -earth complex and preparation method of coated -earth complex
  • Rare-earth complex coated nanometer hollow SiO2, coated -earth complex and preparation method of coated -earth complex
  • Rare-earth complex coated nanometer hollow SiO2, coated -earth complex and preparation method of coated -earth complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1 Rare earth complex Tb(acac) 3 Preparation of phen

[0045] Will Tb 4 o 7 The powder is dissolved in a certain amount of hydrogen peroxide solution, and the product obtained after a period of reaction is filtered and evaporated, then dissolved in dilute hydrochloric acid, and then evaporated slowly until white crystal TbCl appears 3 ·6H 2 O, and then placed in a desiccator for continuous drying until the quality does not change.

[0046] Prepared TbCl 3 ·6H 2 O, acac and phen were dissolved in ethanol to prepare a solution with a certain concentration, and the rare earth complex was prepared according to the TbCl 3 ·6H 2 The molar concentration ratio of O, acac and phen is 1:3:1, and the pH value is adjusted between 7-8.

Embodiment 2

[0047] Example 2 Rare earth complex coated nano hollow SiO 2 preparation of

[0048] The preparation of hollow silica adopts template method.

[0049] (1) Synthetic spherical calcium carbonate: take 50mL concentration to be 0.6mol L -1 Calcium chloride solution, add 100mL of carboxymethylcellulose (CMC) solution with a concentration of 1% and mix evenly, then add sodium carbonate solution with the same volume and concentration as the calcium chloride solution under ultrasonication and stirring, and centrifuge after 10 minutes , the precipitate was washed three times with distilled water and absolute ethanol successively, and dried at 80°C for 24 hours to obtain spherical calcium carbonate;

[0050] (2) Preparation of nanoscale hollow silica particles: Weigh 1 g of the prepared spherical calcium carbonate as a template, add it to a 100 mL round bottom flask, add 30 mL of ethanol, 20 mL of water, 1.0 mL of concentrated ammonia, and 0.10 g of ten Hexaalkyltrimethylammonium bro...

Embodiment 3

[0053] Example 3 SiO 2 @Tb(acac) 3 Fluorescence spectroscopic determination of phen

[0054] Fluorescence spectrum was measured on a fluorescence protractor, and the excitation slit and emission slit were both set to 5nm. In order to more intuitively compare the fluorescence intensity before and after hollow silica embedding, the fluorescence measurement was carried out at the same time and at the same concentration.

[0055] Figure 9 It is a rare earth complex Tb(acac) 3 Hollow silica SiO encapsulated by phen and rare earth complexes 2 @Tb(acac) 3 The emission spectrum of phen is excited with a wavelength of 545nm to obtain the excitation spectrum. Then select the excitation wavelength from the excitation spectrum to obtain the emission spectrum. It can be seen from the figure that both have a very obvious main emission peak at 545nm, and the position of the emission peak does not change much. This shows that the encapsulation of hollow silica has no effect on the ene...

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Abstract

The invention discloses rare-earth complex coated nanometer hollow SiO2. The rare-earth complex coated nanometer hollow SiO2 takes nanometer hollow silicon dioxide as a core, and takes rare-earth complex as a shell to be coated on the surface of the hollow silicon dioxide in an electrostatic adsorption mode, so as to form a particulate material. The rare-earth complex coated nanometer hollow SiO2effectively solves the problems of stability and fluorescence intensity of the rare-earth complex, not only greatly improves the fluorescence intensity of the rare-earth complex of a core-shell structure, but also reduce the dosage of the rare-earth complex. The rare-earth complex coated nanometer hollow SiO2 uses the high biocompatibility of silicon dioxide, and can be applied to biological carriers and fluorescence probes.

Description

technical field [0001] The invention relates to a rare earth complex and hollow silica, in particular to a rare earth complex coated nano hollow SiO 2 And coated rare earth complex and preparation method thereof. It belongs to the field of hybrid materials and their preparation. Background technique [0002] In recent years, research on hollow microspheres has become a research hotspot in the field of materials science. Hollow microspheres with a particle size of nanometer to micrometer have the characteristics of large specific surface area, low density, good stability and filterability, and the hollow part can accommodate a large number of guest molecules or large-sized guests, resulting in some peculiar based on The nature of the microscopic "wrapping" effect. Therefore, as a new type of functional material, hollow microspheres have been widely used in the fields of chemistry, biomedicine and materials, such as catalyst carriers, fillers, coatings, controlled release m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/02C09K11/06C09K11/59B82Y30/00B82Y40/00G01N21/64
CPCB82Y30/00B82Y40/00C09K11/02C09K11/06C09K11/592G01N21/6486
Inventor 王薇李付霞唐建国王瑶王久兴沈文飞李国鹏李磊杨传开
Owner QINGDAO UNIV
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